CN104762053A - Novel multi-purpose fire retardation glue and preparation method thereof - Google Patents

Novel multi-purpose fire retardation glue and preparation method thereof Download PDF

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Publication number
CN104762053A
CN104762053A CN201410013475.4A CN201410013475A CN104762053A CN 104762053 A CN104762053 A CN 104762053A CN 201410013475 A CN201410013475 A CN 201410013475A CN 104762053 A CN104762053 A CN 104762053A
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Prior art keywords
fire retardant
retardant glue
glue
nco
novel fire
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CN201410013475.4A
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Inventor
查玮峰
查忠源
周红兵
万松林
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Wuxi Shuan Mao Novel Material Co Ltd
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Wuxi Shuan Mao Novel Material Co Ltd
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Priority to CN201410013475.4A priority Critical patent/CN104762053A/en
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Abstract

The present invention provides a novel multi-purpose fire retardation glue and a preparation method thereof, wherein the raw materials comprise, by weight, 30-45% of a NCO-based polyurethane prepolymer, 18-30% of a plasticizer, 28-35% of a fire retardation material, 2-5% of a PVC paste resin, 0.5-0.9% of a coupling agent, 0.6-0.9% of a dehydrating agent, and 0.1% of a catalyst, and mixing stirring is performed to obtain the fire retardation glue. The fire retardation glue prepared through the method of the present invention has the following characteristics that: the fire retardation glue has characteristics of no solvent polymer, high solid content, low toxicity, environmental protection, single component, and multi-purpose, the chemical harmful factors are lower than the harmful factor health-based occupational exposure limit, the shelf life is 1 year, the use age can achieve more than or equal to 15 years, the fire retardation glue has good water resistance, can be used for adhesion of various types of warship and ship rigid, semi-rigid, and soft thermal insulation (insulating) materials and warship and ship cabin room wall steel plates, and can adhered with a variety of substrates (including non-polar materials), and the fire retardation oxygen index is more than or equal to 30.0%.

Description

A kind of multipurpose novel fire retardant glue and preparation method thereof
Technical field
The present invention relates to chemical materials and preparation method thereof, is a kind of multipurpose novel fire retardant glue and preparation method thereof specifically.
Background technology
Fire retardant glue is by inorganic raw materials such as aluminium hydroxide, magnesium hydroxide, water glass, fireproofing agent, high molecular polymers, a kind of high molecular fire retardant caking agent formed after High Temperature High Pressure polymerization.It is mainly used in the various structural fire-retardant adhering and sealing having fire-retardant demand in industrial production, as: the structural bond of automobile bodies light plate; CRT picture tube, the insulation of the contour voltage segment of DY deflector coil is bonding and seal; PCB sensor, electric capacity, triode etc. fixing and bonding; Refrigerator, microwave oven, wiring board, electronic devices and components, field of solar energy adhering and sealing; The protection against the tide of exquisite electrical fittings, waterproof enclosure; Automobile headlamp washer sealing; The adhering and sealing reinforcing of wear resistant ceramic chip, window frame mounting glass is pasted in power plant's pipeline; To the elastic adhesive of most metals and non-metallic material, be specially adapted to the elastic adhesive had temperature under particular requirement environment; The bonding reinforcing seal protection of insulation etc. of electric power, electronics, electrical equipment, medical machinery, sensor, mechanical means, refrigerating apparatus, shipbuilding industry, automotive industry, chemical industry light industry, electric wire.
Existing fire retardant glue has certain shortcoming in quality guaranteed period, working life and environmental protection, fire prevention etc.The quality guaranteed period of existing fire retardant glue only has 6 months, and working life is within 10 years, and toxicity level is high, harm large, there is pollution, and flameproof effect is poor simultaneously.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides a kind of multipurpose novel fire retardant glue and preparation method thereof, and the quality guaranteed period of fire retardant glue prepared by this method is 1 year, working life can reach more than 15 years, and toxicity level is low, and harm is few, and energy-conserving and environment-protective, pollution-free, flameproof effect is good.
In order to solve the problems of the technologies described above, the invention provides following technical scheme:
A kind of multipurpose novel fire retardant glue, each weight ratio of constituents is the NCO-base polyurethane prepolymer of 30-45%, the softening agent of 18-30%, the fire retardant material of 28-35%, the PVC paste resin of 2-5%, the coupling agent of 0.5-0.9%, the dewatering agent of 0.6-0.9% and the catalyzer of 0.1%.
Further, in NCO-base polyurethane prepolymer, the mass ratio of polyether glycol, TDI and MDI is 10: 0.8-1.2: 5.
Further, softening agent is the 1-2 kind mixture in o-phthalic acid dibutyl ester or dibutyl phthalate (DBP).
Further, flame retardant materials is the 1-5 kind mixture in magnesium hydroxide, aluminium hydroxide, antimonous oxide, the special halogen-free flame retardants of TPU or silicon-series five-retardant.
Further, if without the need to time fire-retardant, flame retardant materials changes interpolation stopping composition into.
Further, stopping composition is the 1-5 kind mixture in white carbon black, calcium carbonate, talcum powder, clay, mica, calcium sulfate or barium sulfate.
Further, coupling agent is vinyltriethoxysilane.
Further, dewatering agent is the 1-2 kind mixture in calcium chloride, tolysulfonyl isocyanic ester, zeolite activity powder or Benzoyl chloride.
Further, catalyzer is organic tin catalyzer.
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 80-100 DEG C, stir, under vacuum state, obtain polyether glycol; Dehydration 1-3 hour, is cooled to 40 DEG C, adds isocyanic ester, be warming up to 80 DEG C, reaction 2-3 hour, adds catalyzer, continues reaction 1-2 hour, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of the 30-45% in step (1), evenly add the softening agent of 18-30%, the flame retardant materials of 28-35%, the PVC paste resin of 2-5%, the coupling agent of 0.5-0.9%, the dewatering agent of 0.6-0.9% and the catalyst mix of 0.1%, continue under vacuum state to stir 1-2 hour, discharging, can obtain fire retardant glue.
A kind of multipurpose novel fire retardant glue of the present invention and preparation method thereof, fire retardant glue prepared by this method is that highly filled, low toxicity, environmental friendliness, single-component, multi-usage, chemical noxious factor are lower than adverse factor occupational exposure limit; Quality guaranteed period is 1 year, and working life can reach more than 15 years; There is good water tolerance, bonding with between warship, ship stateroom bulkhead steel plate of all kinds of hard in naval vessel, semi-rigid, soft heat insulation (insulation) material can be used in, can be bonding with multiple base material (comprising non-polar material), fire-retardant oxygen index >=30.0%.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Embodiment 1:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 85 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 1 hour, be cooled to 40 DEG C, add isocyanic ester, be warming up to 80 DEG C, react 2 hours, add catalyzer, continue reaction 1 hour, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 30% in step (1), evenly add the o-phthalic acid dibutyl ester of 30%, dibutyl phthalate (DBP) 2 kinds of mixtures, magnesium hydroxide, aluminium hydroxide, antimonous oxide 3 kinds of mixtures of 35%, the PVC paste resin of 3.8%, the vinyltriethoxysilane of 0.5%, the calcium chloride of 0.6%, tolysulfonyl isocyanic ester 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 1 hour under vacuum state, discharging, can obtain fire retardant glue.
Embodiment 2:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 95 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 2 hours, be cooled to 40 DEG C, add isocyanic ester, be warming up to 80 DEG C, react 2 hours, add catalyzer, continue reaction 1 hour, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 40% in step (1), evenly add the o-phthalic acid dibutyl ester of 25%, dibutyl phthalate (DBP) 2 kinds of mixtures, magnesium hydroxide, aluminium hydroxide, the special halogen-free flame retardants of TPU 3 kinds of mixtures of 30%, the PVC paste resin of 3.6%, the vinyltriethoxysilane of 0.6%, the tolysulfonyl isocyanic ester of 0.7%, zeolite activity powder 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 1 hour under vacuum state, discharging, can obtain fire retardant glue.
Embodiment 3:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 100 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 3 hours, be cooled to 40 DEG C, add isocyanic ester, be warming up to 85 DEG C, react 3 hours, add catalyzer, continue reaction 2 hours, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 45% in step (1), evenly add the o-phthalic acid dibutyl ester of 30%, dibutyl phthalate (DBP) 2 kinds of mixtures, magnesium hydroxide, aluminium hydroxide, silicon-series five-retardant 3 kinds of mixtures of 21.1%, the PVC paste resin of 2%, the vinyltriethoxysilane of 0.9%, the zeolite activity powder of 0.9%, calcium chloride 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 2 hours under vacuum state, discharging, can obtain fire retardant glue.
Embodiment 4:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 80 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 2 hours, be cooled to 40 DEG C, add isocyanic ester, be warming up to 80 DEG C, react 3 hours, add catalyzer, continue reaction 2 hours, obtain the NCO-polyurethane prepolymer that content is about 4%-5%, then add micro-Water-free environment-friendlyurinal solvent adjustment viscosity, be down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 30% in step (1), evenly add the o-phthalic acid dibutyl ester of 30%, dibutyl phthalate (DBP) 2 kinds of mixtures, magnesium hydroxide, aluminium hydroxide, antimonous oxide, the special halogen-free flame retardants of TPU 4 kinds of mixtures of 35%, the PVC paste resin of 3.8%, the vinyltriethoxysilane of 0.5%, the calcium chloride of 0.6%, zeolite activity powder 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 1 hour under vacuum state, discharging, can obtain fire retardant glue.
Embodiment 5:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 90 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 1 hour, be cooled to 40 DEG C, add isocyanic ester, be warming up to 85 DEG C, react 2 hours, add catalyzer, continue reaction 1 hour, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 40% in step (1), evenly add the o-phthalic acid dibutyl ester of 25%, dibutyl phthalate (DBP) 2 kinds of mixtures, magnesium hydroxide, aluminium hydroxide, the special halogen-free flame retardants of TPU, silicon-series five-retardant 4 kinds of mixtures of 30%, the PVC paste resin of 3.6%, the vinyltriethoxysilane of 0.6%, the tolysulfonyl isocyanic ester of 0.7%, calcium chloride 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 1 hour under vacuum state, discharging, can obtain fire retardant glue.
Embodiment 6:
A preparation method for multipurpose novel fire retardant glue, its concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 100 DEG C, stir, under vacuum state, obtain polyether glycol; Dewater 2 hours, be cooled to 40 DEG C, add isocyanic ester, be warming up to 85 DEG C, react 2 hours, add catalyzer, continue reaction 2 hours, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of 45% in step (1), evenly add the o-phthalic acid dibutyl ester of 30%, dibutyl phthalate (DBP) 2 kinds of mixtures, the special halogen-free flame retardants of 21.1% magnesium hydroxide, aluminium hydroxide, antimonous oxide, TPU, silicon-series five-retardant 5 kinds of mixtures, the PVC paste resin of 2%, the vinyltriethoxysilane of 0.9%, the zeolite activity powder of 0.9%, tolysulfonyl isocyanic ester 2 kinds of mixtures and 0.1% organic tin catalyst mix, stirring is continued 2 hours under vacuum state, discharging, can obtain fire retardant glue.
The present invention is a kind of multipurpose novel fire retardant glue and preparation method thereof, fire retardant glue prepared by this method can be used in bonding with between warship, ship stateroom bulkhead steel plate of the various types of hard in naval vessel, semi-rigid, soft heat insulation (insulation) material, metallic substance is bonding with fire-retardant (sealing) of non-metallic material junction, appliance electronic component fix and fire-retardant (sealing) bonding, Yi Jijian, portlight frame (doorframe) peripheral rubber sealed strip, circle with the bonding of hull metallic connection parts position and seal use.The maximum feature of this fire retardant glue: the bonding that can be widely used in nonpolar (the being not easy bonding) storerooms such as such as rubber (natural, synthesis) goods, stainless steel, aluminium alloy extrusions, glasswork.And have fire-retardant (sealing) in the engineering construction needing fire-retardant restriction requirement to bond.The establishing criteria of this fire retardant glue cohesive strength: the viscosity (-50 DEG C, 200 DEG C, normal temperature) of GB/T7124-2008 metal foil and nonmetal (glass fibre).The functional performance of this fire retardant glue: highly filled, low toxicity, environmental friendliness, single-component, multi-usage, chemical noxious factor lower than adverse factor occupational exposure limit [" workplace harmful factors occupational exposure limit chemical noxious factor " (GBZ2.1-2007)], [LC 50> 50.0g/m 3for hypotoxicity material (GJB3881)], the LC of this fire retardant glue 50> 94.6g/m 3, belong to lower toxicity material.The physical property of this fire retardant glue: without hazardous solvent volatilization, without dirty gas and VOC discharge, lower chemical noxious factor (i.e. three-waste free discharge).The quality guaranteed period of fire retardant glue prepared by this method is 1 year, and working life can reach more than 15 years; There is good water tolerance, can be bonding with multiple base material thing (containing nonpolar), fire-retardant oxygen index >=30.0%.
Finally, it should be noted that above what enumerate is only 6 kinds of specific embodiments of the present invention.Obviously, the present invention is not limited to above embodiment, can also have a lot of distortion.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention, all should think protection scope of the present invention.

Claims (10)

1. a multipurpose novel fire retardant glue, it is characterized in that: in described multipurpose novel fire retardant glue, each weight ratio of constituents is the NCO-base polyurethane prepolymer of 30-45%, the softening agent of 18-30%, the flame retardant materials of 28-35%, the PVC paste resin of 2-5%, the coupling agent of 0.5-0.9%, the dewatering agent of 0.6-0.9% and the catalyzer of 0.1%.
2. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: in described NCO-base polyurethane prepolymer, the mass ratio of polyether glycol, TDI and MDI is 10: 0.8-1.2: 5.
3. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: described softening agent is the 1-2 kind mixture in o-phthalic acid dibutyl ester or dibutyl phthalate (DBP).
4. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: described flame retardant materials is the 1-5 kind mixture in magnesium hydroxide, aluminium hydroxide, antimonous oxide, the special halogen-free flame retardants of TPU or silicon-series five-retardant.
5. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: if without the need to time fire-retardant, described flame retardant materials changes interpolation stopping composition into.
6. a kind of multipurpose novel fire retardant glue according to claim 5, is characterized in that: described stopping composition is the 1-5 kind mixture in white carbon black, calcium carbonate, talcum powder, clay, mica, calcium sulfate or barium sulfate.
7. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: described coupling agent is vinyltriethoxysilane.
8. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: described dewatering agent is the 1-4 kind mixture in calcium chloride, tolysulfonyl isocyanic ester, zeolite activity powder or Benzoyl chloride.
9. a kind of multipurpose novel fire retardant glue according to claim 1, is characterized in that: described catalyzer is organic tin catalyzer.
10. a preparation method for multipurpose novel fire retardant glue, is characterized in that: concrete steps are as follows:
(1) building-up process of NCO-base polyurethane prepolymer
Under normal temperature, select oxyethane and or the molecular weight that obtains of propylene oxide be 1000 and or 700 macromolecular material compositely join in reactor, be warming up to 80-100 DEG C, stir, under vacuum tightness state, obtain polyether glycol; Dehydration 1-3 hour, is cooled to 40 DEG C, adds isocyanic ester, be warming up to 80 DEG C, reaction 2-3 hour, adds catalyzer, continues reaction 1-2 hour, adjustment content is the NCO-polyurethane prepolymer of about 4%-5%, then adds micro-Water-free environment-friendlyurinal solvent adjustment viscosity, is down to normal temperature.
(2) fire retardant glue is composite
Get the NCO-base polyurethane prepolymer of the 30-45% in step (1), evenly add the softening agent of 18-30%, the fire retardant material of 28-35%, the PVC paste resin of 2-5%, the coupling agent of 0.5-0.9%, the dewatering agent of 0.6-0.9% and the catalyst mix of 0.1%, continue under vacuum state to stir 1-2 hour, discharging, can obtain fire retardant glue.
CN201410013475.4A 2014-01-04 2014-01-04 Novel multi-purpose fire retardation glue and preparation method thereof Pending CN104762053A (en)

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Cited By (8)

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Publication number Priority date Publication date Assignee Title
CN105754538A (en) * 2016-03-23 2016-07-13 烟台信友新材料股份有限公司 Ultraviolet curing adhesive allowing heating curing and preparation method
CN106317854A (en) * 2016-08-24 2017-01-11 广东三和化工科技有限公司 Single-component polyurethane foam joint mixture and preparing method thereof
CN106381074A (en) * 2016-08-30 2017-02-08 无锡万能胶粘剂有限公司 Flame-retardant universal glue
CN108384418A (en) * 2018-02-10 2018-08-10 晋江市永固纺织涂层有限公司 A kind of PU fire retardant glues and its preparation process
CN108485583A (en) * 2018-03-27 2018-09-04 无锡双锚新材料有限公司 Multipurpose fire retardant glue and preparation method thereof, application
CN108913046A (en) * 2018-06-21 2018-11-30 苏州市回天科技有限公司 A kind of fire-retardant tacky film of high elongation rate and preparation method thereof
CN109880576A (en) * 2019-01-24 2019-06-14 深圳市锦昊辉矿业发展有限公司 Single-component moisture curing polyurethane ceramic sealant
CN109913167A (en) * 2019-02-25 2019-06-21 浙江久大纺织科技有限公司 A kind of water-based polyurethane adhesive

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Publication number Priority date Publication date Assignee Title
CN105754538A (en) * 2016-03-23 2016-07-13 烟台信友新材料股份有限公司 Ultraviolet curing adhesive allowing heating curing and preparation method
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CN108485583A (en) * 2018-03-27 2018-09-04 无锡双锚新材料有限公司 Multipurpose fire retardant glue and preparation method thereof, application
CN108913046A (en) * 2018-06-21 2018-11-30 苏州市回天科技有限公司 A kind of fire-retardant tacky film of high elongation rate and preparation method thereof
CN109880576A (en) * 2019-01-24 2019-06-14 深圳市锦昊辉矿业发展有限公司 Single-component moisture curing polyurethane ceramic sealant
CN109913167A (en) * 2019-02-25 2019-06-21 浙江久大纺织科技有限公司 A kind of water-based polyurethane adhesive

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